Acetic Anhydride → Mls000756290

HRID 1729582

반응식

HRID 1729582 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[NH:13][CH2:14][CH3:15])[C:7]([NH2:9])=[O:8])([O-])=O.[C:16](OC(=O)C)(=O)[CH3:17]>[Ni].C(O)(=O)C>[CH2:14]([N:13]1[C:12]2[CH:11]=[CH:10][C:6]([C:7](=[O:8])[NH2:9])=[CH:5][C:4]=2[N:1]=[C:16]1[CH3:17])[CH3:15]

참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 37089224-Ethylamino-3-nitrobenzamide

생성물 1

HCID 292579Mls000756290

시약·촉매·용매 2

HCID 935Nickel촉매HCID 176Acetic Acid용매

실험 절차

A mixture of III (125 g - 0.6 mole), acetic anhydride (214 g - 2.1 moles), Raney Nickel (1.2 ml) and acetic acid (36 g - 0.6 mole) was hydrogenated at 80° C and a pressure of 100 to 30 atm. Reaction time: 5 hours. After cooling, the catalyst was filtered, the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. 150 ml of H2SO4 6N were added to the residue. The reaction was very exothermic. The solution was refluxed with active carbon for 15 min. and filtered. The filtrate was mixed with 1.2 kg of ice and exactly neutralized with 2N NaOH. The precipitate was washed with water and dried at 100° C.

후처리

  1. customwas hydrogenated at 80° C
  2. customReaction time
  3. custom5 hours
  4. temperatureAfter cooling
  5. filtrationthe catalyst was filtered
  6. concentrationthe filtrate was concentrated by normal pressure until 135 ml of distillate
  7. customwere collected
  8. addition150 ml of H2SO4 6N were added to the residue
  9. temperatureThe solution was refluxed with active carbon for 15 min.
  10. filtrationfiltered
  11. additionThe filtrate was mixed with 1.2 kg of ice
  12. washThe precipitate was washed with water
  13. customdried at 100° C.

출처 및 근거

ORD 기록
ord-27961eb4825241f79cc2ef007d9cc5e1
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03989522

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